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Hydrochloride methanol → HCID 21979793, compound

HRID 10493
Notes
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Reaction equation

HRID 10493 reaction equation
C(OC([NH:8][CH2:9][CH2:10][CH2:11][N:12]([S:20]([C:23]1[CH:32]=[CH:31][CH:30]=[C:29]2[C:24]=1[CH:25]=[CH:26][N:27]=[CH:28]2)(=[O:22])=[O:21])[CH2:13][CH2:14][C:15]1[S:16][CH:17]=[CH:18][CH:19]=1)=O)(C)(C)C.[ClH:33].CO>>[ClH:33].[CH:28]1[C:29]2[C:24](=[C:23]([S:20]([N:12]([CH2:13][CH2:14][C:15]3[S:16][CH:17]=[CH:18][CH:19]=3)[CH2:11][CH2:10][CH2:9][NH2:8])(=[O:22])=[O:21])[CH:32]=[CH:31][CH:30]=2)[CH:25]=[CH:26][N:27]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21979924HCID 21979924, compound

Product 1

HCID 21979793HCID 21979793, compound

Procedure

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 3 (238 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with methanol (1 ml) and diethyl ether (3 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (202 mg) as white powdery solid.

Workup

  1. custom(50° C., 2 hours)
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was added with methanol (1 ml) and diethyl ether (3 ml)
custom
The deposited precipitates
  • filtrationwere collected by filtration
  • washwashed with diethyl ether
  • Sources & evidence

    ORD record
    ord-b5e351201461494c8b84873e8fe9cd2a
    Source dataset
    uspto-grants-2006_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US07094789B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes